STUDIES OF PH ZONE REFINING COUNTERCURRENT CHROMATOGRAPHY

PH区精炼逆流色谱研究

• 批准号: 5203506
• 负责人: Y ITO
• 金额: --
• 依托单位: NATIONAL HEART, LUNG, AND BLOOD INSTITUTE
• 依托单位国家: 美国
• 资助国家: 美国
• 起止时间: 至
• 项目状态: 未结题
• 来源: https://reporter.nih.gov/project-details/5203506
• 关键词: acidity /alkalinity; chemical models; hydropathy; mathematical model

Chiral separation of (+/-)-dinitrobenzoyl(DNB) amino acids was successfully performed in both analytical and preparative scales by high-speed CCC, using a chiral selector (CS), N-dodecanoyl-L-proline- 3,5-dimethylanilide. The separations were carried out with a two-phase solvent system composed of hexane/ethyl acetate/ methanol/10mM HCl (8:2:5:5) by adding a proper amount of the CS in the organic stationary phase. The sample size ranging up to 2g was separated in 2-7 hours. Various parameters involved in the chiral resolution were investigated using a set of DNB-amino acid racemates. The results indicated that increasing the concentration of the CS in the stationary phase improves both separation factor (alpha) and peak resolution (Rs). Increasing the hydrophobicity of the solvent system also increased the alpha of the racemate while it affected the peak resolution differently according to the partition coefficient of the racemate. Our results indicated that the best separation will be achieved by applying a high CS concentration and adjusting the hydrophobicity of the solvent system so that the partition coefficient of (K) the racemates falls between 0.6 and 0.8. A simple mathematical analysis on the chiral separation shows good agreement with the experimental data.

研究了（+/-）-二硝基苯甲酰基（DNB）氨基酸对映体的拆分方法， 通过以下方式在分析和制备规模上成功进行 高速CCC，使用手性选择剂（CS），N-十二烷酰基-L-脯氨酸- 3，5-二甲基苯胺。 分离用两相分离器进行。 由己烷/乙酸乙酯/甲醇/10 mM HCl组成的溶剂系统 （8：2：5：5），在有机固定相中加入适量的壳聚糖 相位在2-7小时内分离高达2g的样品量。 考察了手性拆分过程中的各种参数 使用一组DNB-氨基酸外消旋物。 结果表明 增加固定相中CS的浓度 分离因子（α）和峰分离度（Rs）。 增加 溶剂系统的疏水性也增加了 而它对峰分辨率的影响不同， 配分系数。 我们的研究结果表明， 通过应用高CS浓度将实现最佳分离 和调节溶剂体系的疏水性， 外消旋体的分配系数（K）为福尔斯0.6 ~ 0.8。 对手性分离进行了简单的数学分析， 与实验数据一致。

项目成果

Feasibility of multiple short, 40-s, intra-procedural ECG recordings to detect immediate changes in heart rate variability during catheter ablation for arrhythmias.

• DOI: 10.1007/s10840-011-9580-2
• 发表时间: 2011-11
• 期刊: JOURNAL OF INTERVENTIONAL CARDIAC ELECTROPHYSIOLOGY
• 影响因子: 1.8
• 作者: Lim, Phang Boon;Malcolme-Lawes, Louisa C.;Stuber, Thomas;Koa-Wing, Michael;Wright, Ian J.;Tillin, Therese;Sutton, Richard;Davies, D. Wyn;Peters, Nicholas S.;Francis, Darrel P.;Kanagaratnam, Prapa
• 通讯作者: Kanagaratnam, Prapa